#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:37:04 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179193 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/34/4313463.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4313463
loop_
_publ_author_name
'Ricardo González'
'Raúl Chiozzone'
'Carlos Kremer'
'Giovanni De Munno'
'Francesco Nicolò'
'Francesc Lloret'
'Miguel Julve'
'Juan Faus'
_publ_contact_author_address
;    Dip. di Chimica
     Universitá della Calabria
     Arcavacata, Cosenza
     Italy
;
_publ_contact_author_email       demunno@unical.it
_publ_contact_author_fax         39(0984)492088
_publ_contact_author_name        'De Munno, Giovanni'
_publ_contact_author_phone       39(0984)492044
_publ_section_title
;
 Magnetic Studies on Hexaiodorhenate(IV) Salts of Univalent Cations. Spin
 Canting and Magnetic Ordering in K2[ReI6] with Tc= 24 K
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2512
_journal_page_last               2518
_journal_paper_doi               10.1021/ic020531j
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'H8 I6 N2 Re'
_chemical_formula_weight         983.68
_space_group_IT_number           128
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4 2n'
_symmetry_space_group_name_H-M   'P 4/m n c'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   7.8808(11)
_cell_length_b                   7.8808(11)
_cell_length_c                   11.474(2)
_cell_measurement_reflns_used    46
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      14.30
_cell_measurement_theta_min      7.88
_cell_volume                     712.62(19)
_computing_molecular_graphics    'XPW (Siemens, 1996)'
_computing_publication_material  'PARST97 (Nardelli, 1995) and SHELXL-97'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.000
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2θ/ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0829
_diffrn_reflns_av_sigmaI/netI    0.0580
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            1277
_diffrn_reflns_theta_full        0.50
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.14
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    21.478
_exptl_absorpt_correction_T_max  0.0599
_exptl_absorpt_correction_T_min  0.0497
_exptl_crystal_colour            dark-brown
_exptl_crystal_density_diffrn    4.584
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedric
_exptl_crystal_F_000             830
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.542
_refine_diff_density_min         -3.709
_refine_diff_density_rms         0.469
_refine_ls_extinction_coef       0.0031(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     28
_refine_ls_number_reflns         340
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0436
_refine_ls_shift/su_max          0.065
_refine_ls_shift/su_mean         0.014
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0623P)²+9.4834P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1080
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                307
_reflns_number_total             340
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic020531j_1.cif
_cod_data_source_block           compound6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_cell_volume        712.6(2)
_cod_database_code               4313463
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'y-1/2, x-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Re Re 0.0000 0.0000 0.5000 0.0197(5) Uani 1 8 d S . .
I1 I 0.0000 0.0000 0.26278(14) 0.0466(6) Uani 1 4 d S . .
I2 I 0.21243(16) -0.27141(16) 0.5000 0.0416(6) Uani 1 2 d S . .
N N 0.0000 -0.5000 0.7500 0.053(7) Uani 1 4 d SD . .
H1 H 0.069(3) -0.455(5) 0.6784(19) 0.050 Uiso 0.25 1 d PD . .
H2 H -0.1280(12) -0.469(5) 0.740(3) 0.050 Uiso 0.25 1 d PD . .
H3 H 0.046(5) -0.444(5) 0.8260(18) 0.050 Uiso 0.25 1 d PD . .
H4 H 0.013(5) -0.6317(7) 0.756(4) 0.050 Uiso 0.25 1 d PD . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Re 0.0213(6) 0.0213(6) 0.0165(7) 0.000 0.000 0.000
I1 0.0619(9) 0.0619(9) 0.0161(8) 0.000 0.000 0.000
I2 0.0386(8) 0.0329(8) 0.0534(8) 0.000 0.000 0.0154(5)
N 0.055(10) 0.055(10) 0.050(14) 0.000 0.000 -0.021(13)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Re Re -1.0185 7.2310 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
I2 Re I2 90.0 11_556 . ?
I2 Re I2 180.0 11_556 3 ?
I2 Re I2 90.0 . 3 ?
I2 Re I2 90.0 11_556 9_556 ?
I2 Re I2 180.0 . 9_556 ?
I2 Re I2 90.0 3 9_556 ?
I2 Re I1 90.0 11_556 . ?
I2 Re I1 90.0 . . ?
I2 Re I1 90.0 3 . ?
I2 Re I1 90.0 9_556 . ?
I2 Re I1 90.0 11_556 9_556 ?
I2 Re I1 90.0 . 9_556 ?
I2 Re I1 90.0 3 9_556 ?
I2 Re I1 90.0 9_556 9_556 ?
I1 Re I1 180.0 . 9_556 ?
H1 N H2 109.47(12) . . ?
H1 N H3 109.47(12) . . ?
H2 N H3 109.47(12) . . ?
H1 N H4 109.47(12) . . ?
H2 N H4 109.47(12) . . ?
H3 N H4 109.47(12) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Re I2 2.7161(12) 11_556 ?
Re I2 2.7162(12) . ?
Re I2 2.7162(12) 3 ?
Re I2 2.7162(12) 9_556 ?
Re I1 2.7218(17) . ?
Re I1 2.7218(17) 9_556 ?
N H1 1.0448(9) . ?
N H2 1.0448(9) . ?
N H3 1.0448(9) . ?
N H4 1.0448(10) . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N H1 I2 1.04 2.752(9) 3.7783(11) 167(3) .
N H2 I1 1.04 2.953(13) 3.9431(6) 158(3) 13_556
N H3 I2 1.04 2.749(8) 3.7783(11) 168(3) 7_546
N H4 I1 1.04 2.912(9) 3.9431(6) 169(3) 9_546
